TL;DR: In this paper, the order of band gap energy of these samples was found to be rod-shaped > spherical > spindle-like samples, as determined by the UV−Vis spectroscopic method.
Abstract: Spherical cerium oxide nanoparticles and microsized rod-shaped and spindle-like CeO2 structures have been synthesized using a polyol method. When the duration of reaction and the concentration of cerium precursor are controlled, CeO2 products of different morphologies can be selectively produced. Results from XRD, XPS, SEM, and FT-IR measurements suggest that the CeO2 nanospheres are formed from the decomposition of the cerium precursor. Further reactions between the as-prepared CeO2 and ethylene glycol yield the rods/spindle-like cerium formate particles. These morphologies are preserved even after calcination. The order of band gap energy of these samples was found to be rod-shaped > spherical > spindle-like samples, as determined by the UV−Vis spectroscopic method. Compared to a nonoriented polycrystalline CeO2, these samples show an increase in band gap energy due to the quantum size effect. The higher catalytic activity on CO conversion in a spindle-like sample can be explained from the extent of Ce(...
TL;DR: A series of cerium ion-doped titanium dioxide (Ce3+−TiO2) catalysts with special 4f electron configuration was prepared by a sol-gel process and characterized by Brunauer-Emmett-Teller method.
Abstract: A series of cerium ion-doped titanium dioxide (Ce3+–TiO2) catalysts with special 4f electron configuration was prepared by a sol–gel process and characterized by Brunauer-Emmett-Teller method, X-ray diffraction, X-ray photoelectron spectroscopy (XPS), UV–vis diffuse reflectance spectroscopy (DRS), and also photoluminescence (PL) emission spectroscopy. The photocatalytic activity of Ce3+–TiO2 catalysts was evaluated in the 2-mercaptobenzothiazole (MBT) degradation in aqueous suspension under UV or visible light illumination. The experimental results demonstrated that the overall photocatalytic activity of Ce3+–TiO2 catalysts in MBT degradation was signigicantly enhanced due to higher adsorption capacity and better separation of electron-hole pairs. The experimental results verified that both the adsorption equilibrium constant (Ka) and the saturated adsorption amount (Γmax) increased with the increase of cerium ion content. The results of XPS analysis showed that the Ti3+, Ce3+, and Ce4+ ions reside in the Ce3+–TiO2 catalysts. The results of DRS analysis indicated that the Ce3+–TiO2 catalysts had significant optical absorption in the visible region between 400 and 500 nm because electrons could be excited from the valence band of TiO2 or ground state of cerium oxides to Ce 4f level. In the meantime, the dependence of the electron-hole pair separation on cerium ion content was investigated by the PL analysis. It was found that the separation efficiency of electron-hole pairs increased with the increase of cerium ion content at first and then decreased when the cerium ion content exceeded its optimal value. It is proposed that the formation of two sub-energy levels (defect level and Ce 4f level) in Ce3+–TiO2 might be a critical reason to eliminate the recombination of electron-hole pairs and to enhance the photocatalytic activity.
TL;DR: A series of cerium ion-doped titanium dioxide (Ce 3+ -TiO2) catalysts with special 4 f electron configuration was prepared by a sol-gel process and characterized by Brunauer-Emmett-Teller method as discussed by the authors.
Abstract: A series of cerium ion-doped titanium dioxide (Ce 3+ –TiO2) catalysts with special 4 f electron configuration was prepared by a sol–gel process and characterized by Brunauer-Emmett-Teller method, X-ray diffraction, X-ray photoelectron spectroscopy (XPS), UV–vis diffuse reflectance spectroscopy (DRS), and also photoluminescence (PL) emission spectroscopy. The photocatalytic activity of Ce 3+ –TiO2 catalysts was evaluated in the 2-mercaptobenzothiazole (MBT) degradation in aqueous suspension under UV or visible light illumination. The experimental results demonstrated that the overall photocatalytic activity of Ce 3+ –TiO2 catalysts in MBT degradation was signigicantly enhanced due to higher adsorption capacity and better separation of electron-hole pairs. The experimental results verified that both the adsorption equilibrium constant (Ka) and the saturated adsorption amount (Gmax) increased with the increase of cerium ion content. The results of XPS analysis showed that the Ti 3+ ,C e 3+ , and Ce 4+ ions reside in the Ce 3+ –TiO2 catalysts. The results of DRS analysis indicated that the Ce 3+ –TiO2 catalysts had significant optical absorption in the visible region between 400 and 500 nm because electrons could be excited from the valence band of TiO2 or ground state of cerium oxides to Ce 4 f level. In the meantime, the dependence of the electron-hole pair separation on cerium ion content was investigated by the PL analysis. It was found that the separation efficiency of electron-hole pairs increased with the increase of cerium ion content at first and then decreased when the cerium ion content exceeded its optimal value. It is proposed that the formation of two sub-energy levels (defect level and Ce 4 f level) in Ce 3+ –TiO2 might be a critical reason to eliminate the recombination of
TL;DR: In this paper, Lanthanide-promoted sol-gel nickel catalysts supported on alumina were studied with regard to their activity and stability for propane steam reforming, showing that adding small amounts (2 wt%) of lanthanide elements (i.e., La, Ce, and Yb) significantly improves steam reforming activity.
TL;DR: In this article, the influence of supporting oxides on the structural and redox properties of CeO2 were systematically investigated by various techniques namely, X-ray diffraction (XRD), Raman spectroscopy (RS), UV-Vis diffuse reflectance spectrograph (DRS) and high-resolution transmission electron microscopy (HREM), and thermogravimetry methods.
Abstract: The influence of SiO2, TiO2, and ZrO2 on the structural and redox properties of CeO2 were systematically investigated by various techniques namely, X-ray diffraction (XRD), Raman spectroscopy (RS), UV–Vis diffuse reflectance spectroscopy (DRS), X-ray photoelectron spectroscopy (XPS), high-resolution transmission electron microscopy (HREM), BET surface area, and thermogravimetry methods. The effect of supporting oxides on the crystal modification of ceria was also mainly focused. The investigated oxides were obtained by soft chemical routes with ultrahigh dilute solutions and were subjected to thermal treatments from 773 to 1073 K. The XRD results suggest that the CeO2–SiO2 sample primarily consists of nanocrystalline CeO2 on the amorphous SiO2 surface. Both crystalline CeO2 and TiO2-anatase phases were noted in the case of CeO2–TiO2 sample. Formation of cubic Ce0.75Zr0.25O2 and Ce0.6Zr0.4O2 (at 1073 K) were observed in the case of CeO2–ZrO2 sample. The cell ‘a’ parameter estimations revealed an expansion of the ceria lattice in the case of CeO2–TiO2, while a contraction is noted in the case of CeO2–ZrO2. The DRS studies suggest that the supporting oxides significantly influence the band gap energy of CeO2. Raman measurements disclose the presence of oxygen vacancies, lattice defects, and displacement of oxide ions from their normal lattice positions in the case of CeO2–TiO2 and CeO2–ZrO2 samples. The XPS studies revealed the presence of silica, titania, and zirconia in their highest oxidation states, Si(IV), Ti(IV), and Zr(IV) at the surface of the materials. Cerium is present in both Ce4+ and Ce3+ oxidation states. The HREM results reveal well-dispersed CeO2 nanocrystals over the amorphous SiO2 matrix in the case of CeO2–SiO2, isolated CeO2 and TiO2 (A) nanocrystals and some overlapping regions in the case of CeO2–TiO2, and nanosized CeO2 and Ce–Zr oxides in the case of CeO2–ZrO2 sample. The exact structural features of these crystals as determined by digital diffraction analysis of HREM experimental images reveal that the CeO2 is mainly in cubic fluorite geometry. The oxygen storage capacity (OSC) as determined by thermogravimetry reveals that the OSC of mixed oxides is more than that of pure CeO2 and the CeO2–ZrO2 exhibits highest OSC.
TL;DR: Well-crystalline CeO(2-x) nanotubes are synthesized via a mild hydrothermal reaction route using cerium nitrate and ammonium hydroxide as reactants.
Abstract: Well-crystalline CeO2-x nanotubes are synthesized via a mild hydrothermal reaction route using cerium nitrate and ammonium hydroxide as reactants. The CeO2-x nanotubes have the same structure as the bulk CeO2 but larger lattice parameter. The measurement of the ratio of M5/M4 edge shows the valence reduction of cerium ions for the CeO2-x nanotubes.
TL;DR: In this paper, the effects of starting cerium compounds, hydrothermal treatment temperature, and the concentration of the solutions on the crystal growth of CeO 2 were investigated, and mechanisms for the growth of C 2 particles under hydrothermally conditions were discussed.
Abstract: CeO 2 powders have been prepared from cerium(III) nitrate, cerium(IV) sulfate, and cerium(IV) ammonium sulfate under hydrothermal conditions at 120° to 200°C for 5 to 40 h. The effects of the starting cerium compounds, hydrothermal treatment temperature, and the concentration of the solutions on the crystal growth of CeO 2 were investigated. Ceo 2 powders hydrothermally synthesized at 180°C for 5 h from cerium(IV) salts had very fine particle sizes (30 A) ; on the other hand, the powder from the cerium(III) salt had a relatively coarse particle size (160 A). Although the crystallite size of the powder synthesized from the cerium(IV) compounds depended on the treatment temperature, that from the cerium(III) compound was insensitive to the treatment temperature. The mechanisms for the growth of CeO 2 particles under hydrothermal conditions are discussed.
TL;DR: In this article, the effects brought about by the cerium salt precursor ((NH 4 ) 2 Ce(NO 3 ) 6 or Ce( NO 3 ) 3 ), the introduction of drying and aging steps as well as pH controlling upon precipitation were analyzed.
Abstract: The preparation of CeO 2 –ZrO 2 mixed oxides preparation was studied by evaluating the influence of several conditions Coprecipitation was taken as the standard method and the effects brought about by the cerium salt precursor ((NH 4 ) 2 Ce(NO 3 ) 6 or Ce(NO 3 ) 3 ), the introduction of drying and aging steps as well as pH controlling upon precipitation were analyzed The samples were characterized by X-ray diffraction, Raman spectroscopy, temperature-programmed reduction, infrared spectroscopy, oxygen storage capacity and surface area The use of Ce(NO 3 ) 3 leads to the formation of c -CeO 2 and t -ZrO 2 mixed oxide whereas a solid solution is achieved by using (NH 4 ) 2 Ce(NO 3 ) 6 It was observed that the cerium precursor is the most significant parameter of preparation procedure since it defines the crystalline phases and consequently the reducibility behavior of the CeO 2 –ZrO 2 system
TL;DR: The antineoplastic potential of cerium compounds, which had fallen into oblivion, is currently being re-explored in experimental settings, though the mechanistic basis remains to be elucidated.
Abstract: Cerium is a member of the lanthanide series or rare earth elements which exert diverse biological effects mainly by their resemblance to calcium. This similarity, which is particularly characteristic for the lighter members of the lanthanide series, enables these elements to replace calcium in biomolecules without necessarily substituting for it functionally. While the inhibitory effects on calcium-dependent physiological processes (such as those involved in the blood clotting cascade as well as in neuronal and muscular functions) are well-known, their relevance for the pharmacological properties of cerium are less clear. Historically, cerium oxalate was used as an antiemetic, especially in vomiting of pregnancy and kinetoses, although its mechanism of action has never been clarified. At present, cerium nitrate is available as an adjunct to silver sulfadiazine cream for the topical treatment of extensive burns not amenable to early wound excision. Apart from direct antiseptic effects, cerium helps to prevent postburn sepsis and systemic inflammatory response by fixing burn toxins. The antineoplastic potential of cerium compounds, which had fallen into oblivion, is currently being re-explored in experimental settings, though the mechanistic basis remains to be elucidated.
TL;DR: In this paper, a cryptomelane type manganese oxide OMS-2 material was synthesized by redox reaction between potassium permanganate and Manganese sulphate in acidic medium under reflux or hydrothermal crystallization conditions.
Abstract: Cryptomelane type manganese oxide OMS-2 material was synthesized by redox reaction between potassium permanganate and manganese sulphate in acidic medium under reflux or hydrothermal crystallization conditions. Ce was added by ion-exchange, impregnation or directly at crystallization stage. The chemical composition, structure, texture, morphology and thermal stability of the materials were measured by EDX spectroscopy, XRD, N 2 -adsorption, SEM and TGA. Results of the catalytic wet oxidation of phenol at 100 °C indicate best performance of the well-crystallized octahedral molecular sieve with cryptomelane structure where all the accessible potassium ions were exchanged for cerium cations. OMS-2 materials containing pure CeO 2 phase and excess of active oxygen species had lower stability, activity and capacity for oxidative reactive adsorption of phenol. Implementation of Ce-exchanged crystalline OMS-2 catalyst improves the wastewater treatment capacity by a factor of 1.5–2 and 3 compared with co-precipitated Mn–Ce-oxide and activated carbon, respectively.
TL;DR: HT materials were synthesized by several methods including cerium addition and it was demonstrated that the isomorphic incorporation of iron increased its reduction capability which was reflected in higher reduction rates and metal sulfate reduction grade at 550 degrees C.
Abstract: Sulfur oxides are one of the most hazardous atmospheric pollutants since they contribute directly to acid rain formation. Consequently, stringent environmental regulations limit atmospheric SOx emissions, motivating research on efficient ways to reduce them. To supply an alternative to reduce these emissions in fluid catalytic cracking units, this study discloses efficient SOx reducing materials based on calcined MgAlFe hydrotalcite-like compounds (HT's). Thus, HT materials were synthesized by several methods including cerium addition. The adsorption of SO2 was carried out by contacting the calcined solid with a mixture of SO2 (1%) in air at 650 °C. It was demonstrated that the isomorphic incorporation of iron increased its reduction capability which was reflected in higher reduction rates and metal sulfate reduction grade at 550 °C. Moreover, when cerium was present in the iron-containing materials the saturation rate was improved, because cerium oxide promotes the oxidation of SO2 to SO3. The way cerium...
TL;DR: In this paper, the luminescence properties of ZnS nanoparticles are greatly affected by either the microwave irradiation time or dopants of various metallic ions (Ag +, Cu 2+, Ce 3+ and Sn 4+ ).
TL;DR: In this article, X-ray absorption spectroscopy at the Ce LIII-edge was applied for the characterization of crystalline anhydrous cerium(III) nitrate, nanocrystalline hydrous and amorphous cerium oxides.
Abstract: Cerium oxide solid samples were prepared via precipitation from aqueous solution of hydrous cerium(III) nitrate in the presence of different percentages of hydrogen peroxide (H2O2) as model corrosion inhibiting coatings materials for aluminum alloys. X-ray absorption spectroscopy at the Ce LIII-edge was applied for the characterization of crystalline anhydrous CeO2, nanocrystalline hydrous CeO2, nanocrystalline CeO2 sample I precipitated in the presence of H2O2, and an amorphous CeO2 sample II precipitated at a higher H2O2 concentration. An analysis by X-ray absorption near-edge structure (XANES) for cerium oxides did not indicate a broad variation in cerium valence state in the precipitated samples as compared to anhydrous CeO2. Furthermore, XANES analysis revealed a decrease in the intensity of the white line peaks for the precipitated samples relative to those in anhydrous CeO2. The EXAFS spectra of the oxides showed that H2O2 reduced the precipitate's particle diameter and bulk crystallinity. Growth i...
TL;DR: The Gd-doped cerium dioxides, which can be modified with Pt or Pd to enhance the reactivity of the lattice oxygen in interaction with methane, are studied to elucidate correlations between the structural, electronic, and chemical properties of these nanomaterials.
Abstract: Nanostructured ceria doped with other rare earth elements is a good oxygen ion conductor, which gives rise to various catalytic applications such as the construction of membranes for syngas production by partial oxidation of methane. This article focuses on the Gd-doped cerium dioxides, which can be modified with Pt or Pd to enhance the reactivity of the lattice oxygen in interaction with methane. The aim of the work is the elucidation of correlations between the structural, electronic, and chemical properties of these nanomaterials. Detailed studies were performed for a series of samples with and without surface modification by noble metals using a complex combination of physicochemical methods: XRD, TEM, CH4 TPR, XPS, SIMS, and FTIR spectroscopy of adsorbed CO. XPS and TPR data revealed that surface modification with noble metals enhances the reducibility of the doped ceria support, where the effect is more pronounced for Pd than for Pt. The formation of highly cationic Pd species due to strong metal s...
TL;DR: In this paper, Pectin-based cerium (IV) and thorium-IV phosphates have been synthesized as new phases of hybrid fibrous ion exchangers, and both materials were characterized using X-ray diffraction, infrared (IR) spectra, thermogravimetric analysis (TG), differntial thermograimetry (DTG), differentntial thermal analysis (DTA), and scanning electron microscopy (SEM), as well as the determination of their ion exchange capacity, elution and pH titration.
Abstract: Pectin based cerium (IV) and thorium (IV) phosphates have been synthesized as new phases of hybrid fibrous ion exchangers. Both materials were characterized using X-ray diffraction, infrared (IR) spectra, thermogravimetric analysis (TG), differntial thermogravimetry (DTG), differntial thermal analysis (DTA) and scanning electron microscopy (SEM), as well as the determination of their ion exchange capacity, elution and pH titration. The X-ray study reveals the amorphous nature of the materials, while SEM studies confirm the fibrous nature of the materials. The thermal studies of these materials indicate that both of them are highly stable on heating as they retain about 97% of their ion-exchange capacity (i.e.c.) on heating up to 100°C and about 81% on heating up to 200°C.
TL;DR: The homogeneous rare-earth dispersion in the host matrix and the stabilization of the Ce(3+) oxidation state enhanced the intensity of the photoluminescence emission in PSG and BPSG with respect to BSG and SG.
Abstract: Ce-doped borosilicate (BSG), phosphosilicate (PSG), and borophosphosilicate (BPSG) glasses (B:P:Si molar ratios 8:0:92, 0:8:92, and 8:8:84; Ce:Si molar ratio 1 x 10(-)(4) to 1 x 10(-)(2)) were prepared by the sol-gel method. High-resolution transmission electron microscopy (HRTEM), (31)P, (29)Si, and (11)B magic angle spinning nuclear magnetic resonance (MAS NMR), electron paramagnetic resonance (EPR), and UV-vis absorption investigations demonstrated that, in PSG and BPSG, Ce(3+) ions interact with phosphoryl, [O=PO(3/2)], metaphosphate, [O=PO(2/ 2)O](-), and pyrophosphate, [O=PO(1/2)O(2)](2)(-), groups, linked to a silica network. This inhibits both CeO(2) segregation and oxidation of isolated Ce(3+) ions to Ce(4+), up to Ce:Si = 5 x 10(-)(3). In BSG, neither trigonal [BO(3/2)] nor tetrahedral [BO(4/2)](-) boron units coordinate cerium; thus, Ce(3+) oxidation occurs even at Ce:Si = 1 x 10(-)(4), as in pure silica glass (SG). The homogeneous rare-earth dispersion in the host matrix and the stabilization of the Ce(3+) oxidation state enhanced the intensity of the photoluminescence emission in PSG and BPSG with respect to BSG and SG. The energy of the Ce(3+) emission band in PSG and BPSG matrixes agrees with the phosphate environment of the rare earth.
TL;DR: In this article, high-homogeneous (Ce,Tb) oxides are prepared by a micro-emulsion technique, and their structural and electronic state after high temperature calcination is examined with X-ray diffraction, high resolution transmission electron microscopy, X -ray photoelectron and absorption (XANES) spectroscopies and impedance spectroscopy measurements.
TL;DR: The results showed that in this composition range the apatite structure is maintained, Ce3 + ions could enter the crystal lattice of ap atite and substitute Ca2 + ions.
Abstract: The aim of this study was to explore the effect of cerium ions on the formation and structure of hydroxyapatite (HAP). All particles, prepared by hydrothermal method, were synthesized at varied XCe = Ce/(Ca + Ce) (from 0 to 10%) with the atomic ratio (Ce + Ca)/P fixed at 1.67. Their morphology, composition and crystal structure were characterized by TEM, EPMA, XRD and FTIR. The results showed that in this composition range the apatite structure is maintained, Ce3 + ions could enter the crystal lattice of apatite and substitute Ca2 + ions. The doping of Ce3 + ions resulted in the decrease of the crystallite size with increase in XCe. The HAP particles without doping were short rods having a diameter from 10 to 20 nm and a length from 30 to 50 nm. They grew into long needles upon increasing XCe.
TL;DR: In this paper, the authors proposed a protocol for regioselective iodization of a wide range of aromatic compounds with sodium iodide in the presence of the easily prepared, water-resistant and recyclable cerium(IV) trihydroxide hydroperoxide, Ce(OH)3O2H, at room temperature.
Abstract: Micellar solutions of sodium dodecyl sulfate (SDS) catalyze the regioselective iodination of a wide range of aromatic compounds with sodium iodide in the presence of the easily prepared, water-resistant and recyclable cerium(IV) trihydroxide hydroperoxide, Ce(OH)3O2H, at room temperature. By this protocol, structurally diverse aromatic compounds including benzene and naphthalene were iodinated in good to excellent yields.
TL;DR: Corrosion inhibition of aluminum alloy (AA)2024-T3 (UNS A92024) in sodium chloride (NaCl) solutions after pretreatments in solutions containing Ce(III), Co(II), or Mo(VI) ions are reported.
Abstract: Corrosion inhibition of aluminum alloy (AA)2024-T3 (UNS A92024) in sodium chloride (NaCl) solutions after pretreatments in solutions containing Ce(III), Co(II), or Mo(VI) ions are reported
TL;DR: In this paper, a single-phase α-Ce 2 S 3 powder was formed via sulfurization at 973 K for 28.8 ks, and the data of densification by hot pressing was analyzed by a kinetic equation that was proposed by other researchers.
Abstract: Cerium(III) sulfide (Ce 2 S 3 ) powder was synthesized via the sulfurization of ceria (CeO 2 ) powder using carbon disulfide gas. Single-phase α-Ce 2 S 3 could be formed via sulfurization at 973 K for 28.8 ks. The preparation of α-Ce 2 S 3 became feasible at low temperature, in comparison to sulfurization using hydrogen sulfide gas. According to the fact that the formation of α-Ce 2 S 3 was accelerated by the addition of carbon black to the CeO 2 powder, carbothermic reduction was considered to become a dominant reaction, as the temperature increased. To obtain the activation energy for the densification of β-Ce 2 S 3 powder, which was prepared by vacuum heating α-Ce 2 S 3 , the data of densification by hot pressing was analyzed by a kinetic equation that was proposed by other researchers. As a result, the sintering behavior could be best explained by a grain-boundary-diffusion mechanism that had an apparent activation energy of 382 kJ/mol.
TL;DR: In this article, the crystal structure, thermal stability, textural property and morphology of OMS-2 catalysts have been characterized using XRD, TGA, BET and TEM techniques.
TL;DR: Five psychoactive drugs, namely, chlorpromazine HCl, thioridazine Hcl, clomipramine H Cl, imipramsine HCl and desipramines HCl were analyzed by a simple spectrofluorimetric method based on oxidation of the studied drugs using cerium(IV) in presence of sulphuric acid.
TL;DR: In this paper, the stability and nature of metal−ligand multiple bonding between the tetravalent lanthanide element cerium and a number of different ligand sets that commonly form met...
TL;DR: In this paper, the surfaces of ceria (CeO 2 ) particles have been studied by electron energy-loss spectroscopy in a field-emission gun scanning transmission electron microscope.
TL;DR: In this article, the effect of cerium on the properties of zirconia-supported platinum catalysts was studied in the water gas shift reaction (WGSR) at high temperatures (320-450°C) over hematite-based catalysts doped with chromium.
TL;DR: In this paper, a highly effective, economical, and environmentally friendly method using of CAN as oxidant and water as solvent for oxidative coupling of N,N-dialkylarylamines was reported.
TL;DR: In this paper, a cerium-zirconium-base composite oxide was proposed for the purification of exhaust gas discharged from combustion engines such as internal combustion engines and boilers and can release a high level of oxygen in a low temperature region.
Abstract: This invention relates to a cerium-zirconium-base composite oxide, which is useful, e.g., for the purification of exhaust gas discharged from combustion engines such as internal combustion engines and boilers and can release a high level of oxygen in a low temperature region, a method for producing the same, an oxygen storage/release component using the same, an exhaust gas purification catalyst, and an exhaust gas purification method. The cerium-zirconium-base composite oxide satisfies requirements (1) that the oxygen release initiation temperature is 380° C. or below, (2) that the oxygen release amount is not less than 485 μmol/g, and further (3) that the oxygen release amount at 400° C. is not less than 15 μmol/g. The cerium-zirconium-base composite oxide can be produced, for example, by mixing a starting material for cerium and a starting material for zirconium at a predetermined mixing ratio together, melting the starting material mixture at a temperature at or above the melting point, then cooling the melt to form an ingot, then optionally grinding the ingot to prepare powder, subsequently removing strain within powder crystal grains under heating, and then grinding to a further fine state.